#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/55/2225564.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2225564
loop_
_publ_author_name
'Lin, Pei-Xi'
'Yang, Gui-Bin'
'An, Zhe'
_publ_section_title
;
 Di-μ-sulfato-κ⁴O:O'-bis{bis[3-(2-pyridyl)pyrazole]cobalt(II)}
;
_journal_coeditor_code           HB5349
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m375
_journal_paper_doi               10.1107/S160053681000797X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co2 (S O4)2 (C8 H7 N3)4]'
_chemical_formula_moiety         'C32 H28 Co2 N12 O8 S2'
_chemical_formula_sum            'C32 H28 Co2 N12 O8 S2'
_chemical_formula_weight         890.64
_chemical_name_systematic
;
Di-μ-sulfato-κ⁴O:O'-bis{bis[3-(2-pyridyl)pyrazole]cobalt(II)}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.342(8)
_cell_angle_beta                 98.820(9)
_cell_angle_gamma                99.302(8)
_cell_formula_units_Z            1
_cell_length_a                   8.318(5)
_cell_length_b                   9.879(5)
_cell_length_c                   11.807(6)
_cell_measurement_reflns_used    3228
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.14
_cell_volume                     925.1(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0108
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4790
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.543
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0780P)²+1.7757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                2990
_reflns_number_total             3228
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb5349.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        925.2(9)
_cod_database_code               2225564
_cod_database_fobs_code          2225564
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.42221(5) 0.79964(4) 0.84355(4) 0.03040(18) Uani d . 1 . .
C C1 -0.0398(5) 0.9232(4) 0.7050(3) 0.0420(9) Uani d . 1 . .
H H1 -0.1395 0.9531 0.7097 0.050 Uiso calc R 1 . .
C C2 0.0198(5) 0.8857(4) 0.6063(3) 0.0448(9) Uani d . 1 . .
H H2 -0.0302 0.8835 0.5298 0.054 Uiso calc R 1 . .
C C3 0.1714(4) 0.8511(4) 0.6431(3) 0.0318(7) Uani d . 1 . .
C C4 0.2985(4) 0.8065(4) 0.5790(3) 0.0371(8) Uani d . 1 . .
C C5 0.2946(6) 0.8116(6) 0.4641(4) 0.0636(13) Uani d . 1 . .
H H5 0.2092 0.8431 0.4223 0.076 Uiso calc R 1 . .
C C6 0.4197(7) 0.7690(8) 0.4113(4) 0.090(2) Uani d . 1 . .
H H6 0.4207 0.7721 0.3332 0.108 Uiso calc R 1 . .
C C7 0.5414(7) 0.7226(7) 0.4750(4) 0.0846(19) Uani d . 1 . .
H H7 0.6261 0.6922 0.4406 0.102 Uiso calc R 1 . .
C C8 0.5382(5) 0.7212(5) 0.5893(4) 0.0530(11) Uani d . 1 . .
H H8 0.6220 0.6890 0.6322 0.064 Uiso calc R 1 . .
C C9 0.8750(4) 0.6412(4) 0.9368(4) 0.0403(8) Uani d . 1 . .
H H9 0.9883 0.6490 0.9619 0.048 Uiso calc R 1 . .
C C10 0.7598(4) 0.5198(3) 0.9034(3) 0.0368(8) Uani d . 1 . .
H H10 0.7774 0.4287 0.9004 0.044 Uiso calc R 1 . .
C C11 0.6107(4) 0.5620(3) 0.8748(3) 0.0249(6) Uani d . 1 . .
C C12 0.4408(4) 0.4824(3) 0.8353(3) 0.0252(6) Uani d . 1 . .
C C13 0.4011(4) 0.3396(3) 0.8316(3) 0.0342(7) Uani d . 1 . .
H H13 0.4828 0.2898 0.8524 0.041 Uiso calc R 1 . .
C C14 0.2386(5) 0.2743(4) 0.7967(4) 0.0490(10) Uani d . 1 . .
H H14 0.2081 0.1786 0.7933 0.059 Uiso calc R 1 . .
C C15 0.1224(5) 0.3493(4) 0.7670(4) 0.0517(10) Uani d . 1 . .
H H15 0.0114 0.3059 0.7434 0.062 Uiso calc R 1 . .
C C16 0.1705(4) 0.4906(4) 0.7721(3) 0.0425(8) Uani d . 1 . .
H H16 0.0898 0.5414 0.7512 0.051 Uiso calc R 1 . .
N N1 0.0705(3) 0.9095(3) 0.7943(2) 0.0293(6) Uani d . 1 . .
H H1A 0.0596 0.9270 0.8664 0.035 Uiso calc R 1 . .
N N2 0.2007(3) 0.8649(3) 0.7574(2) 0.0283(6) Uani d . 1 . .
N N3 0.4193(4) 0.7642(3) 0.6426(2) 0.0355(6) Uani d . 1 . .
N N4 0.7960(3) 0.7468(3) 0.9271(2) 0.0298(6) Uani d . 1 . .
H H4 0.8437 0.8338 0.9435 0.036 Uiso calc R 1 . .
N N5 0.6333(3) 0.7005(3) 0.8887(2) 0.0249(5) Uani d . 1 . .
N N6 0.3280(3) 0.5577(3) 0.8057(2) 0.0294(6) Uani d . 1 . .
O O1 0.1481(3) 0.9642(2) 1.03701(19) 0.0307(5) Uani d . 1 . .
O O2 0.4260(3) 1.0067(3) 1.1403(3) 0.0592(9) Uani d . 1 . .
O O3 0.2278(3) 0.8263(3) 1.1747(2) 0.0411(6) Uani d . 1 . .
O O4 0.3184(3) 0.7973(3) 0.9944(2) 0.0429(6) Uani d . 1 . .
S S1 0.28057(8) 0.89939(7) 1.08803(6) 0.0206(2) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Co1 O4 2_677 . 109.51(13) ?
O2 Co1 N5 2_677 . 92.56(11) ?
O4 Co1 N5 . . 99.64(10) ?
O2 Co1 N2 2_677 . 93.38(11) ?
O4 Co1 N2 . . 89.94(10) ?
N5 Co1 N2 . . 166.34(10) ?
O2 Co1 N6 2_677 . 161.04(12) ?
O4 Co1 N6 . . 83.92(10) ?
N5 Co1 N6 . . 71.51(10) y
N2 Co1 N6 . . 100.13(10) ?
O2 Co1 N3 2_677 . 87.49(13) ?
O4 Co1 N3 . . 155.57(11) ?
N5 Co1 N3 . . 96.88(10) ?
N2 Co1 N3 . . 71.12(10) y
N6 Co1 N3 . . 84.40(10) ?
N1 C1 C2 . . 107.2(3) ?
N1 C1 H1 . . 126.4 ?
C2 C1 H1 . . 126.4 ?
C1 C2 C3 . . 105.4(3) ?
C1 C2 H2 . . 127.3 ?
C3 C2 H2 . . 127.3 ?
N2 C3 C2 . . 110.2(3) ?
N2 C3 C4 . . 117.7(3) ?
C2 C3 C4 . . 132.1(3) ?
N3 C4 C5 . . 122.7(3) ?
N3 C4 C3 . . 114.8(3) ?
C5 C4 C3 . . 122.5(3) ?
C4 C5 C6 . . 118.6(4) ?
C4 C5 H5 . . 120.7 ?
C6 C5 H5 . . 120.7 ?
C7 C6 C5 . . 119.0(4) ?
C7 C6 H6 . . 120.5 ?
C5 C6 H6 . . 120.5 ?
C8 C7 C6 . . 119.3(4) ?
C8 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
N3 C8 C7 . . 122.5(4) ?
N3 C8 H8 . . 118.7 ?
C7 C8 H8 . . 118.7 ?
N4 C9 C10 . . 107.6(3) ?
N4 C9 H9 . . 126.2 ?
C10 C9 H9 . . 126.2 ?
C9 C10 C11 . . 104.7(3) ?
C9 C10 H10 . . 127.7 ?
C11 C10 H10 . . 127.7 ?
N5 C11 C10 . . 110.9(3) ?
N5 C11 C12 . . 117.4(3) ?
C10 C11 C12 . . 131.7(3) ?
N6 C12 C13 . . 122.9(3) ?
N6 C12 C11 . . 115.1(3) ?
C13 C12 C11 . . 122.0(3) ?
C14 C13 C12 . . 118.1(3) ?
C14 C13 H13 . . 121.0 ?
C12 C13 H13 . . 121.0 ?
C15 C14 C13 . . 119.7(3) ?
C15 C14 H14 . . 120.1 ?
C13 C14 H14 . . 120.1 ?
C14 C15 C16 . . 119.2(4) ?
C14 C15 H15 . . 120.4 ?
C16 C15 H15 . . 120.4 ?
N6 C16 C15 . . 122.7(4) ?
N6 C16 H16 . . 118.7 ?
C15 C16 H16 . . 118.7 ?
C1 N1 N2 . . 111.2(3) ?
C1 N1 H1A . . 124.4 ?
N2 N1 H1A . . 124.4 ?
C3 N2 N1 . . 106.0(3) ?
C3 N2 Co1 . . 119.5(2) ?
N1 N2 Co1 . . 134.3(2) ?
C4 N3 C8 . . 117.8(3) ?
C4 N3 Co1 . . 116.2(2) ?
C8 N3 Co1 . . 125.5(2) ?
C9 N4 N5 . . 111.4(3) ?
C9 N4 H4 . . 124.3 ?
N5 N4 H4 . . 124.3 ?
C11 N5 N4 . . 105.3(2) ?
C11 N5 Co1 . . 119.8(2) ?
N4 N5 Co1 . . 134.78(19) ?
C16 N6 C12 . . 117.4(3) ?
C16 N6 Co1 . . 126.2(2) ?
C12 N6 Co1 . . 115.8(2) ?
S1 O2 Co1 . 2_677 153.33(18) ?
S1 O4 Co1 . . 137.65(16) ?
O3 S1 O2 . . 110.08(18) ?
O3 S1 O4 . . 108.22(15) ?
O2 S1 O4 . . 110.2(2) ?
O3 S1 O1 . . 110.61(15) ?
O2 S1 O1 . . 109.36(15) ?
O4 S1 O1 . . 108.40(14) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O2 2_677 2.074(3) y
Co1 O4 . 2.097(3) y
Co1 N5 . 2.187(3) y
Co1 N2 . 2.212(3) y
Co1 N6 . 2.331(3) y
Co1 N3 . 2.331(3) y
C1 N1 . 1.329(4) ?
C1 C2 . 1.351(5) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.386(5) ?
C2 H2 . 0.9300 ?
C3 N2 . 1.312(4) ?
C3 C4 . 1.469(5) ?
C4 N3 . 1.328(4) ?
C4 C5 . 1.362(5) ?
C5 C6 . 1.376(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.357(7) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.357(6) ?
C7 H7 . 0.9300 ?
C8 N3 . 1.336(5) ?
C8 H8 . 0.9300 ?
C9 N4 . 1.332(4) ?
C9 C10 . 1.363(5) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.384(5) ?
C10 H10 . 0.9300 ?
C11 N5 . 1.327(4) ?
C11 C12 . 1.463(4) ?
C12 N6 . 1.332(4) ?
C12 C13 . 1.387(4) ?
C13 C14 . 1.366(5) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.351(6) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.376(6) ?
C15 H15 . 0.9300 ?
C16 N6 . 1.334(4) ?
C16 H16 . 0.9300 ?
N1 N2 . 1.337(4) ?
N1 H1A . 0.8600 ?
N4 N5 . 1.336(4) ?
N4 H4 . 0.8600 ?
O1 S1 . 1.466(2) ?
O2 S1 . 1.446(3) ?
O2 Co1 2_677 2.074(3) ?
O3 S1 . 1.436(2) ?
O4 S1 . 1.466(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A O1 . 0.86 1.98 2.772(4) 152
N4 H4 O1 2_677 0.86 1.96 2.761(4) 155
